반응 #409101

반응 방정식

n-BuLi

4,7-dimethyl indene

4,7-dimethylindene

water

→

1-(4,7-dimethyl-1-indenyl)-2-(4,7-dimethyl-1-indenyl)methyl benzene

용매

THF hexane

—

mixture

hexane

THF hexane

반응 조건

후처리

1. 1
   workup.ADDITIONAt the end of the addition
2. 2
   workup.WAITthe mixture is left
3. 3
   workup.ADDITIONare added dropwise
4. 4
   workup.WAITThe mixture is left
5. 5
   기타to rise to room temperature
6. 6
   workup.WAITis left
7. 7
   workup.WAITto rest for 6 hours
8. 8
   추출is extracted with ethyl ether
9. 9
   세척The organic phase is washed until neutrality
10. 10
    기타The residue obtained by evaporation of the solvent
11. 11
    기타is purified by silica gel chromatography
12. 12
    기타After evaporation of the eluant 2.0 g of the bis-indenyl ligand
13. 13
    기타are obtained (72% yield)

실험 절차

4.12 ml (10.3 mmoles) of n-BuLi 2.5 M in hexane are added to a solution of 1.48 g of 4,7-dimethyl indene (XVIII) (10.3 mmoles; obtained as described above) in 55 ml of a mixture of THF-hexane 2/1. At the end of the addition, the mixture is left under stirring for 1 hour. It is then cooled to −70° C. and a solution of 2.3 g of the brominated compound having formula (XX) (7.37 mmoles) in THF/hexane are added dropwise. The mixture is left to rise to room temperature and is left to rest for 6 hours. It is then poured into water and is extracted with ethyl ether. The organic phase is washed until neutrality and dehydrated on sodium sulfate. The residue obtained by evaporation of the solvent is purified by silica gel chromatography eluating with petroleum ether. After evaporation of the eluant 2.0 g of the bis-indenyl ligand having formula (XXI) and indicated below, are obtained (72% yield).

출처